Bromoacetic Acid → HCID 10633915、化合物

HRID 2187537ノート

反応式

HRID 2187537 の反応式
Cl[S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][C:13]=1[CH:14]([CH3:16])[CH3:15])[C:8]([OH:10])=[O:9])(=[O:4])=[O:3].[CH:17](C1C=CC(C(O)=O)=CC=1)(C)C.C([O-])(O)=O.[Na+].[O-]S([O-])=O.[Na+].[Na+].BrCC(O)=O.[OH-].[Na+]>O>[CH3:17][S:2]([C:5]1[CH:6]=[C:7]([CH:11]=[CH:12][C:13]=1[CH:14]([CH3:16])[CH3:15])[C:8]([OH:10])=[O:9])(=[O:4])=[O:3]

参加物

8

反応物 6

HCID 6227Bromoacetic AcidHCID 108204-Isopropylbenzoic AcidHCID 14798Sodium HydroxideHCID 24437Sodium SulfiteHCID 3095103-(Chlorosulfonyl)-4-(propan-2-yl)benzoic acidHCID 516892Sodium Bicarbonate

生成物 1

HCID 10633915HCID 10633915、化合物収率 59%

試薬・触媒・溶媒 1

HCID 962Water溶媒

反応条件

温度
105 °C

実験手順

3-Chlorosulfonyl-4-iso-propylbenzoic acid (2.62 g, 10 mmol) [made from 4-iso-propyl benzoic acid in a manner similar to that described in Procedures 7 and 8] was added slowly to a slurry of NaHCO3 (2.52 g, 30 mmol) and Na2SO3 (1.26 g 10 mmol) in water (9 ml) at 75° C. The mixture was stirred for 1 h and then treated with bromoacetic acid (2.08 g, 15 mmol) and NaOH (0.60 g, 15 mmol). The temperature was raised to 105° C. and the mixture heated at reflux for 24 h. The mixture was cooled, acidified to pH 1 and the resultant precipitate collected, washed and dried to give the title compound (1.43 g, 59%).

後処理

  1. temperaturethe mixture heated
  2. temperatureat reflux for 24 h
  3. temperatureThe mixture was cooled
  4. customthe resultant precipitate collected
  5. washwashed
  6. customdried

出典と根拠

ORDレコード
ord-3551547cda7c48319ac70129621aca81
出典データセット
uspto-grants-2002_06
特許番号
US06410555B1

反応ノート

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